TW201100330A - Fabrication method for chalcopyrite powder - Google Patents
Fabrication method for chalcopyrite powder Download PDFInfo
- Publication number
- TW201100330A TW201100330A TW098121317A TW98121317A TW201100330A TW 201100330 A TW201100330 A TW 201100330A TW 098121317 A TW098121317 A TW 098121317A TW 98121317 A TW98121317 A TW 98121317A TW 201100330 A TW201100330 A TW 201100330A
- Authority
- TW
- Taiwan
- Prior art keywords
- preparing
- chalcopyrite
- powder according
- group
- compound
- Prior art date
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- 239000000843 powder Substances 0.000 title claims abstract description 91
- 238000000034 method Methods 0.000 title claims abstract description 56
- DVRDHUBQLOKMHZ-UHFFFAOYSA-N chalcopyrite Chemical compound [S-2].[S-2].[Fe+2].[Cu+2] DVRDHUBQLOKMHZ-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 229910052951 chalcopyrite Inorganic materials 0.000 title claims abstract description 53
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 8
- 150000001875 compounds Chemical class 0.000 claims abstract description 41
- 238000010438 heat treatment Methods 0.000 claims abstract description 29
- 239000002243 precursor Substances 0.000 claims abstract description 28
- 238000001035 drying Methods 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 15
- 239000000203 mixture Substances 0.000 claims abstract description 14
- 239000002904 solvent Substances 0.000 claims abstract description 14
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 22
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 18
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 17
- 230000008569 process Effects 0.000 claims description 16
- 239000007789 gas Substances 0.000 claims description 14
- 238000000576 coating method Methods 0.000 claims description 13
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 12
- 239000010949 copper Substances 0.000 claims description 12
- 239000011669 selenium Substances 0.000 claims description 12
- XTEGARKTQYYJKE-UHFFFAOYSA-M Chlorate Chemical compound [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 claims description 10
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims description 10
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 10
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 8
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 claims description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 239000012298 atmosphere Substances 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 7
- 239000011248 coating agent Substances 0.000 claims description 7
- 239000001257 hydrogen Substances 0.000 claims description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims description 7
- 229910021653 sulphate ion Inorganic materials 0.000 claims description 7
- 229940093476 ethylene glycol Drugs 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 5
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 5
- 229910052802 copper Inorganic materials 0.000 claims description 5
- 229910052733 gallium Inorganic materials 0.000 claims description 5
- 235000006408 oxalic acid Nutrition 0.000 claims description 5
- 239000012985 polymerization agent Substances 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 4
- 229910002651 NO3 Inorganic materials 0.000 claims description 4
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 4
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 4
- 239000010931 gold Substances 0.000 claims description 4
- 229910052738 indium Inorganic materials 0.000 claims description 4
- 150000004767 nitrides Chemical class 0.000 claims description 4
- 229910052711 selenium Inorganic materials 0.000 claims description 4
- 229910052717 sulfur Inorganic materials 0.000 claims description 4
- 239000011593 sulfur Substances 0.000 claims description 4
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 3
- 229910019142 PO4 Inorganic materials 0.000 claims description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 3
- 150000001412 amines Chemical class 0.000 claims description 3
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 3
- 238000003618 dip coating Methods 0.000 claims description 3
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 3
- 239000010452 phosphate Substances 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- 238000001556 precipitation Methods 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- 238000005507 spraying Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 2
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 claims description 2
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 2
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 2
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 2
- 239000011358 absorbing material Substances 0.000 claims description 2
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 239000001569 carbon dioxide Substances 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 238000004108 freeze drying Methods 0.000 claims description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052737 gold Inorganic materials 0.000 claims description 2
- 238000007756 gravure coating Methods 0.000 claims description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 2
- 150000002602 lanthanoids Chemical group 0.000 claims description 2
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 2
- 239000011976 maleic acid Substances 0.000 claims description 2
- 229910000069 nitrogen hydride Inorganic materials 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- 239000011591 potassium Substances 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- 238000004528 spin coating Methods 0.000 claims description 2
- 238000004544 sputter deposition Methods 0.000 claims description 2
- 239000011975 tartaric acid Substances 0.000 claims description 2
- 235000002906 tartaric acid Nutrition 0.000 claims description 2
- 229910052714 tellurium Inorganic materials 0.000 claims description 2
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 claims description 2
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 2
- 239000004202 carbamide Substances 0.000 claims 2
- GHVNFZFCNZKVNT-UHFFFAOYSA-N decanoic acid Chemical compound CCCCCCCCCC(O)=O GHVNFZFCNZKVNT-UHFFFAOYSA-N 0.000 claims 2
- 102000040717 Alpha family Human genes 0.000 claims 1
- 108091071248 Alpha family Proteins 0.000 claims 1
- 239000005632 Capric acid (CAS 334-48-5) Substances 0.000 claims 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims 1
- 229930013930 alkaloid Natural products 0.000 claims 1
- 150000001336 alkenes Chemical class 0.000 claims 1
- 229910052782 aluminium Inorganic materials 0.000 claims 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims 1
- 238000005576 amination reaction Methods 0.000 claims 1
- DQLATGHUWYMOKM-UHFFFAOYSA-L cisplatin Chemical compound N[Pt](N)(Cl)Cl DQLATGHUWYMOKM-UHFFFAOYSA-L 0.000 claims 1
- 229960004316 cisplatin Drugs 0.000 claims 1
- RCJVRSBWZCNNQT-UHFFFAOYSA-N dichloridooxygen Chemical compound ClOCl RCJVRSBWZCNNQT-UHFFFAOYSA-N 0.000 claims 1
- 238000001704 evaporation Methods 0.000 claims 1
- 230000008020 evaporation Effects 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims 1
- 238000007641 inkjet printing Methods 0.000 claims 1
- 229910052744 lithium Inorganic materials 0.000 claims 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 claims 1
- 230000000379 polymerizing effect Effects 0.000 claims 1
- 150000003346 selenoethers Chemical class 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 230000003637 steroidlike Effects 0.000 claims 1
- 238000010345 tape casting Methods 0.000 claims 1
- 230000001376 precipitating effect Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 20
- -1 chalcopyrite compound Chemical class 0.000 description 14
- 239000007864 aqueous solution Substances 0.000 description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 8
- 238000002441 X-ray diffraction Methods 0.000 description 8
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 235000015165 citric acid Nutrition 0.000 description 5
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 5
- 150000003431 steroids Chemical class 0.000 description 5
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 4
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 4
- 238000000498 ball milling Methods 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 4
- 239000011780 sodium chloride Substances 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- PPQREHKVAOVYBT-UHFFFAOYSA-H dialuminum;tricarbonate Chemical compound [Al+3].[Al+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O PPQREHKVAOVYBT-UHFFFAOYSA-H 0.000 description 3
- CHPZKNULDCNCBW-UHFFFAOYSA-N gallium nitrate Inorganic materials [Ga+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O CHPZKNULDCNCBW-UHFFFAOYSA-N 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 150000002576 ketones Chemical class 0.000 description 3
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 description 3
- 239000005416 organic matter Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 3
- KPZGRMZPZLOPBS-UHFFFAOYSA-N 1,3-dichloro-2,2-bis(chloromethyl)propane Chemical compound ClCC(CCl)(CCl)CCl KPZGRMZPZLOPBS-UHFFFAOYSA-N 0.000 description 2
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- LCTONWCANYUPML-UHFFFAOYSA-N Pyruvic acid Chemical compound CC(=O)C(O)=O LCTONWCANYUPML-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 229910000420 cerium oxide Inorganic materials 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 2
- MWKFXSUHUHTGQN-UHFFFAOYSA-N decan-1-ol Chemical compound CCCCCCCCCCO MWKFXSUHUHTGQN-UHFFFAOYSA-N 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 2
- 229910000154 gallium phosphate Inorganic materials 0.000 description 2
- LWFNJDOYCSNXDO-UHFFFAOYSA-K gallium;phosphate Chemical compound [Ga+3].[O-]P([O-])([O-])=O LWFNJDOYCSNXDO-UHFFFAOYSA-K 0.000 description 2
- 150000004820 halides Chemical class 0.000 description 2
- PSCMQHVBLHHWTO-UHFFFAOYSA-K indium(iii) chloride Chemical compound Cl[In](Cl)Cl PSCMQHVBLHHWTO-UHFFFAOYSA-K 0.000 description 2
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 2
- PHTQWCKDNZKARW-UHFFFAOYSA-N isoamylol Chemical compound CC(C)CCO PHTQWCKDNZKARW-UHFFFAOYSA-N 0.000 description 2
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- SQDFHQJTAWCFIB-UHFFFAOYSA-N n-methylidenehydroxylamine Chemical compound ON=C SQDFHQJTAWCFIB-UHFFFAOYSA-N 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 2
- SCVFZCLFOSHCOH-UHFFFAOYSA-M potassium acetate Chemical compound [K+].CC([O-])=O SCVFZCLFOSHCOH-UHFFFAOYSA-M 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 238000004626 scanning electron microscopy Methods 0.000 description 2
- 239000013049 sediment Substances 0.000 description 2
- 235000017281 sodium acetate Nutrition 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 2
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 1
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 description 1
- BZSXEZOLBIJVQK-UHFFFAOYSA-N 2-methylsulfonylbenzoic acid Chemical compound CS(=O)(=O)C1=CC=CC=C1C(O)=O BZSXEZOLBIJVQK-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 description 1
- 241000544061 Cuculus canorus Species 0.000 description 1
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- XOBKSJJDNFUZPF-UHFFFAOYSA-N Methoxyethane Chemical compound CCOC XOBKSJJDNFUZPF-UHFFFAOYSA-N 0.000 description 1
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 1
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- RAOSIAYCXKBGFE-UHFFFAOYSA-K [Cu+3].[O-]P([O-])([O-])=O Chemical compound [Cu+3].[O-]P([O-])([O-])=O RAOSIAYCXKBGFE-UHFFFAOYSA-K 0.000 description 1
- KTSFMFGEAAANTF-UHFFFAOYSA-N [Cu].[Se].[Se].[In] Chemical compound [Cu].[Se].[Se].[In] KTSFMFGEAAANTF-UHFFFAOYSA-N 0.000 description 1
- SOQNHTGSYONFGX-UHFFFAOYSA-K [In+3].[O-][Cl](=O)=O.[O-][Cl](=O)=O.[O-][Cl](=O)=O Chemical compound [In+3].[O-][Cl](=O)=O.[O-][Cl](=O)=O.[O-][Cl](=O)=O SOQNHTGSYONFGX-UHFFFAOYSA-K 0.000 description 1
- 150000001242 acetic acid derivatives Chemical class 0.000 description 1
- BGYBTGDDOPTJSB-UHFFFAOYSA-N acetic acid;ethane-1,2-diol Chemical compound CC(O)=O.OCCO BGYBTGDDOPTJSB-UHFFFAOYSA-N 0.000 description 1
- 238000003483 aging Methods 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
- 229940118662 aluminum carbonate Drugs 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- NWAIGJYBQQYSPW-UHFFFAOYSA-N azanylidyneindigane Chemical compound [In]#N NWAIGJYBQQYSPW-UHFFFAOYSA-N 0.000 description 1
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 description 1
- 229910001863 barium hydroxide Inorganic materials 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- ZCLVNIZJEKLGFA-UHFFFAOYSA-H bis(4,5-dioxo-1,3,2-dioxalumolan-2-yl) oxalate Chemical compound [Al+3].[Al+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O ZCLVNIZJEKLGFA-UHFFFAOYSA-H 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 229910000416 bismuth oxide Inorganic materials 0.000 description 1
- MNBLRJWKVLRTKV-UHFFFAOYSA-N bromo selenohypobromite Chemical compound Br[Se]Br MNBLRJWKVLRTKV-UHFFFAOYSA-N 0.000 description 1
- 229910052792 caesium Inorganic materials 0.000 description 1
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 description 1
- 235000013877 carbamide Nutrition 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- XTEGARKTQYYJKE-UHFFFAOYSA-N chloric acid Chemical compound OCl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-N 0.000 description 1
- 229940005991 chloric acid Drugs 0.000 description 1
- SWAKCLHCWHYEOW-UHFFFAOYSA-N chloro selenohypochlorite Chemical compound Cl[Se]Cl SWAKCLHCWHYEOW-UHFFFAOYSA-N 0.000 description 1
- 150000001860 citric acid derivatives Chemical class 0.000 description 1
- 238000010549 co-Evaporation Methods 0.000 description 1
- 229940125898 compound 5 Drugs 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229940116318 copper carbonate Drugs 0.000 description 1
- 229910000365 copper sulfate Inorganic materials 0.000 description 1
- 229910000153 copper(II) phosphate Inorganic materials 0.000 description 1
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 1
- 229910000366 copper(II) sulfate Inorganic materials 0.000 description 1
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 description 1
- GEZOTWYUIKXWOA-UHFFFAOYSA-L copper;carbonate Chemical compound [Cu+2].[O-]C([O-])=O GEZOTWYUIKXWOA-UHFFFAOYSA-L 0.000 description 1
- IJCCOEGCVILSMZ-UHFFFAOYSA-L copper;dichlorate Chemical compound [Cu+2].[O-]Cl(=O)=O.[O-]Cl(=O)=O IJCCOEGCVILSMZ-UHFFFAOYSA-L 0.000 description 1
- AEJIMXVJZFYIHN-UHFFFAOYSA-N copper;dihydrate Chemical compound O.O.[Cu] AEJIMXVJZFYIHN-UHFFFAOYSA-N 0.000 description 1
- QYCVHILLJSYYBD-UHFFFAOYSA-L copper;oxalate Chemical compound [Cu+2].[O-]C(=O)C([O-])=O QYCVHILLJSYYBD-UHFFFAOYSA-L 0.000 description 1
- RGZGHMSJVAQDQO-UHFFFAOYSA-L copper;selenate Chemical compound [Cu+2].[O-][Se]([O-])(=O)=O RGZGHMSJVAQDQO-UHFFFAOYSA-L 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- FYWVTSQYJIPZLW-UHFFFAOYSA-K diacetyloxygallanyl acetate Chemical compound [Ga+3].CC([O-])=O.CC([O-])=O.CC([O-])=O FYWVTSQYJIPZLW-UHFFFAOYSA-K 0.000 description 1
- VBXWCGWXDOBUQZ-UHFFFAOYSA-K diacetyloxyindiganyl acetate Chemical compound [In+3].CC([O-])=O.CC([O-])=O.CC([O-])=O VBXWCGWXDOBUQZ-UHFFFAOYSA-K 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 description 1
- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 description 1
- ABFDJEJZFDLFAD-UHFFFAOYSA-H digallium;triselenate Chemical compound [Ga+3].[Ga+3].[O-][Se]([O-])(=O)=O.[O-][Se]([O-])(=O)=O.[O-][Se]([O-])(=O)=O ABFDJEJZFDLFAD-UHFFFAOYSA-H 0.000 description 1
- USIUVYZYUHIAEV-UHFFFAOYSA-N diphenyl ether Chemical compound C=1C=CC=CC=1OC1=CC=CC=C1 USIUVYZYUHIAEV-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 229910001195 gallium oxide Inorganic materials 0.000 description 1
- 229910000373 gallium sulfate Inorganic materials 0.000 description 1
- UPWPDUACHOATKO-UHFFFAOYSA-K gallium trichloride Chemical compound Cl[Ga](Cl)Cl UPWPDUACHOATKO-UHFFFAOYSA-K 0.000 description 1
- SBDRYJMIQMDXRH-UHFFFAOYSA-N gallium;sulfuric acid Chemical compound [Ga].OS(O)(=O)=O SBDRYJMIQMDXRH-UHFFFAOYSA-N 0.000 description 1
- 210000004907 gland Anatomy 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 210000000003 hoof Anatomy 0.000 description 1
- 239000004021 humic acid Substances 0.000 description 1
- OAKJQQAXSVQMHS-UHFFFAOYSA-N hydrazine Substances NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 1
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 229910003437 indium oxide Inorganic materials 0.000 description 1
- UJXZVRRCKFUQKG-UHFFFAOYSA-K indium(3+);phosphate Chemical compound [In+3].[O-]P([O-])([O-])=O UJXZVRRCKFUQKG-UHFFFAOYSA-K 0.000 description 1
- DONSDNATLFRYPO-UHFFFAOYSA-H indium(3+);triselenate Chemical compound [In+3].[In+3].[O-][Se]([O-])(=O)=O.[O-][Se]([O-])(=O)=O.[O-][Se]([O-])(=O)=O DONSDNATLFRYPO-UHFFFAOYSA-H 0.000 description 1
- 229910000337 indium(III) sulfate Inorganic materials 0.000 description 1
- IGUXCTSQIGAGSV-UHFFFAOYSA-K indium(iii) hydroxide Chemical compound [OH-].[OH-].[OH-].[In+3] IGUXCTSQIGAGSV-UHFFFAOYSA-K 0.000 description 1
- XGCKLPDYTQRDTR-UHFFFAOYSA-H indium(iii) sulfate Chemical compound [In+3].[In+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O XGCKLPDYTQRDTR-UHFFFAOYSA-H 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052747 lanthanoid Inorganic materials 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- XIXADJRWDQXREU-UHFFFAOYSA-M lithium acetate Chemical compound [Li+].CC([O-])=O XIXADJRWDQXREU-UHFFFAOYSA-M 0.000 description 1
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 1
- 229910052808 lithium carbonate Inorganic materials 0.000 description 1
- XQHAGELNRSUUGU-UHFFFAOYSA-M lithium chlorate Chemical compound [Li+].[O-]Cl(=O)=O XQHAGELNRSUUGU-UHFFFAOYSA-M 0.000 description 1
- INHCSSUBVCNVSK-UHFFFAOYSA-L lithium sulfate Inorganic materials [Li+].[Li+].[O-]S([O-])(=O)=O INHCSSUBVCNVSK-UHFFFAOYSA-L 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- YWWNNLPSZSEZNZ-UHFFFAOYSA-N n,n-dimethyldecan-1-amine Chemical compound CCCCCCCCCCN(C)C YWWNNLPSZSEZNZ-UHFFFAOYSA-N 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 238000005121 nitriding Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 235000011056 potassium acetate Nutrition 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- VKJKEPKFPUWCAS-UHFFFAOYSA-M potassium chlorate Chemical compound [K+].[O-]Cl(=O)=O VKJKEPKFPUWCAS-UHFFFAOYSA-M 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 239000004323 potassium nitrate Substances 0.000 description 1
- 235000010333 potassium nitrate Nutrition 0.000 description 1
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 1
- 229910052939 potassium sulfate Inorganic materials 0.000 description 1
- 235000011151 potassium sulphates Nutrition 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 235000019260 propionic acid Nutrition 0.000 description 1
- 229940107700 pyruvic acid Drugs 0.000 description 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229910000058 selane Inorganic materials 0.000 description 1
- 229940082569 selenite Drugs 0.000 description 1
- MCAHWIHFGHIESP-UHFFFAOYSA-L selenite(2-) Chemical compound [O-][Se]([O-])=O MCAHWIHFGHIESP-UHFFFAOYSA-L 0.000 description 1
- 229910000338 selenium disulfide Inorganic materials 0.000 description 1
- VIDTVPHHDGRGAF-UHFFFAOYSA-N selenium sulfide Chemical compound [Se]=S VIDTVPHHDGRGAF-UHFFFAOYSA-N 0.000 description 1
- VTQZBGAODFEJOW-UHFFFAOYSA-N selenium tetrabromide Chemical compound Br[Se](Br)(Br)Br VTQZBGAODFEJOW-UHFFFAOYSA-N 0.000 description 1
- LNBXMNQCXXEHFT-UHFFFAOYSA-N selenium tetrachloride Chemical compound Cl[Se](Cl)(Cl)Cl LNBXMNQCXXEHFT-UHFFFAOYSA-N 0.000 description 1
- IYKVLICPFCEZOF-UHFFFAOYSA-N selenourea Chemical compound NC(N)=[Se] IYKVLICPFCEZOF-UHFFFAOYSA-N 0.000 description 1
- CQLFBEKRDQMJLZ-UHFFFAOYSA-M silver acetate Chemical compound [Ag+].CC([O-])=O CQLFBEKRDQMJLZ-UHFFFAOYSA-M 0.000 description 1
- 229940071536 silver acetate Drugs 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- 239000004317 sodium nitrate Substances 0.000 description 1
- 235000010344 sodium nitrate Nutrition 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 150000004763 sulfides Chemical class 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 150000004772 tellurides Chemical class 0.000 description 1
- PTYIPBNVDTYPIO-UHFFFAOYSA-N tellurium tetrabromide Chemical compound Br[Te](Br)(Br)Br PTYIPBNVDTYPIO-UHFFFAOYSA-N 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
- 150000003672 ureas Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/007—Tellurides or selenides of metals
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/002—Compounds containing, besides selenium or tellurium, more than one other element, with -O- and -OH not being considered as anions
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S977/00—Nanotechnology
- Y10S977/70—Nanostructure
- Y10S977/813—Of specified inorganic semiconductor composition, e.g. periodic table group IV-VI compositions
- Y10S977/814—Group IV based elements and compounds, e.g. CxSiyGez, porous silicon
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S977/00—Nanotechnology
- Y10S977/70—Nanostructure
- Y10S977/813—Of specified inorganic semiconductor composition, e.g. periodic table group IV-VI compositions
- Y10S977/815—Group III-V based compounds, e.g. AlaGabIncNxPyAsz
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Photovoltaic Devices (AREA)
Abstract
Description
201100330 六、發明說明： 【發明所屬之技術領域】 本發明係有關於一種半導體材料之製法，且特別是有關於一 種黄銅礦（chalcopyrite)粉末之製法。 • 【先前技術】 半導體村料具有彳奇殊的能階大小（band gap) ’可藉由调控材料 組成而改變半導體之能隙，因此可將其應用作為光電元件 (photoelectronic device)之光吸收層。 〇 於各種半導體材料中，其中以具有黃銅礦（chalcopyrite)結構 的I Β-ΠΑ-VIA族化合物特別受到重視，其可製成薄膜應用於硒 化銅銦鎵電池（Cu(In,Ga)Se2, CIGS)中，且具有不錯的光電轉換效 率。 目前製作黃銅礦（c.halcopyrite)化合物之薄膜的方法可分為真 空和非真空製程，真空製程包括共蒸鐘（co-evaporation)、濺鐘 (sputter)等製程，而非真空製程包括電沉積（electrodeposition)、無 電極電锻(electroless)、塗佈製程（coating process)或化學喷霧熱裂 解法（chemical spray p3，rolysis)，由於真空製程製程成本與設備車交 為昂貴，且其僅能應用於小尺寸（small-scale)的光電元件，無法應 用於大尺寸的元件，因此，開始發展非真空技術。 早期非真空製程的製備方法，係分別將I B族與ΠΙΑ族之金 屬離子沉積於基材上，經還原成金屬後，再經過硒化熱處理得到 黃銅礦化合物，然而1ΠΑ族金屬熔點較低，於熱處理過程會因熔 化而聚集（aggregate)，因此會得到不均勻的薄膜。為了得到更為均 勻的薄膜，開始發展各種黃銅礦化合物之製備方式。 US 5,445,847揭露一種製備黃銅礦（chalcopyrite)化合物之方 201100330 法，首先混合IB粉末和HA粉末，之後進行球磨混合後，再送入 高溫燒結（sinter)得到I Β-ΠΙ Α氧化物，最後再經由含有VIA族氣 體中熱處理，即可得到黄銅礦化合物。 US 6,268,014揭露一種黄銅礦化合物之方法，首先製作 IB-ΠΙΛ氧化物顆粒，再利用喷灑方式（spray)沉積於基材上，最 . 後再經由含有VIA族氣體中熱處理，即可得到黄銅礦化合物。 綜上所述，若能製作出一種顆粒小且均勻的黄銅礦化合物之 粉末，將此粉末製成漿料（slmry)後，應用於塗佈製程時即可製作 出均勻的薄膜。 〇 【發明内容】 本發明提供一種黃銅礦（chalcopyrite)粉末之製法，包括以下 步驟：（a)混合含有IB族與ΜΑ族之化合物於一溶劑中；（b)將 步驟（a)之溶液進行一乾燥或沉殿步驟以獲得一含有IB族、IE A族 之前驅物（precursor) ; (c)將一含有VIA族化合物之溶液或粉末與 該前驅物混合；以及（d)將步驟（c)之混合物進行熱處理以得到該 黃銅礦粉末。 本發明另外提供一種黄銅礦（chalcopyrite)粉末之製法，包括 ◎ 以下步驟：（a)混合含有IB族、ΠΙΑ族與VIA族之化合物於一溶 劑中；（b)將步驟（a)之溶液進行一乾燥或沉澱步驟以獲得一含有 IB族、II A族與VIA族之前驅物（precursor);以及（c)將步驟(b) 之前驅物進行熱處理以得到該黃銅礦粉末。 為讓本發明之上述和其他目的、特徵、和優點能更明顯易懂， 下文特舉出較佳實施例，並配合所附圖式，作詳細說明如下： 【實施方式】 4 201100330 本發明提供一種黃銅礦（chaleopyrite)粉末之製法，包括以下 步驟：首先進行步驟（a) ’混合含有IB族與ΠΙA族離子之化合物於 〉谷劑中’其中I B知包括銅（Cu)、銀(Ag)、金(Au)或上述之組合， 而I B族之化合物包括含有I B族之氧化物、氮化物、氳氧化物、 鹵化物、硝酸物、醋酸物、硫酸物、碳酸物、氣酸物、填酸物、 砸酸物、草酸物、填化物’例如氧化銅（CuO)、氮化銅（Cu(N3)2)、 氫氧化銅（Cu(OH)2)、氯化銅（CuCl2)、硝酸銀（AgN03)、硝酸銅 (Cu(N03)2)、硫酸銅（CuS〇4)、醋酸銅（Cu(CH3COO)2)、醋酸銀 (CH3COOAg)、碳酸銅（Cu2C03)、草酸銅（CuC204)、氯酸銅 O (Cu(C104)2)、磷酸銅（Cu3(P04)2)、硒酸銅（CuSe04)或磷化銅（Cu3P)。 ΠΙ A族包括銘（A1)、銦（In)、鎵（Ga)或上述之組合，而皿A族 化合物包括含有H A族之氧化物、氮化物、氫氧化物、化物、 硝酸物、醋酸物、硫酸物、碳酸物、氯酸物、磷酸物、硒酸物' 草酸物或磷化物，例如氧化銦（In2〇3)、氧化鎵（Gar〇3)、氮化銦 (InN)、氮化鎵(GaN)、氫氧化銦（ln(〇H)3)、氫氧化錁(Ga(〇H)3)、 氯化鋁（A1C13)、氯化銦（InCl3)、氯化鎵（GaCl3)、硝酸鋁（A1(N03)3)、 石肖酉文銦（In(N〇3)3)、項酸叙（Ga(N〇3)3)、醋酸銦（ln(CH3COO)3)、酷 Q 酸紹（A1(CH3C00)3)、碳酸鋁（Al2(C〇3)3)、草酸鋁（Al2(C2〇4)3)、醋 酸鎵（Ga(CH3COO)3)、硫酸銦（ln2(s〇4)3)、硫酸鋁（Al2(s〇4)3)、硫 酸鎵(GaKSOO3)、氯酸銦（In(C104)3)、氯酸鎵(Ga(ci〇4)3)、磷酸銦 (ΙηΡ04)、磷酸鎵（GaP04)、硒酸銦（In2(Se〇4)3)、硒酸鎵 (Ga2(Se04)3)、磷化!因(InP)或石粦化鎵(GaP)。 步驟（a)之I B族、HIA族化合物之莫耳數比為約（〇 7〜14): (0.7〜1.4) ’較佳為約（0.8〜1.3) : (0.8〜1.3)，最佳為約（〇.8〜1.2): (0‘8〜1.2)。 而I B族、ΠΙΑ族化合物之選擇，並不限於上述提及之化合 5 201100330 物，只要含有ib族、Ha族元素之化合物皆可。而溶劑包括水、 酸類、鹼類、醇類、酮類、醚類、胺類或其它有機溶劑，這些溶 劑為無毒性之一般溶劑，其中酸類包括硝酸、鹽酸、硫酸、醋酸 或丙酮酸；鹼類包括氫氧化鈉溶液或檸檬酸溶液、氨水；醇類包 括曱醇、乙醇、丙醇、異丙醇、正丁醇、異戊醇或乙二醇；酮類 包括丙酮、丁酮、甲基異丁酮；醚類包括曱醚、乙醚、甲乙醚、 一苯醚、乙一醇曱醚乙一醇丁趟或乙二醇乙醋酸；胺類包括 乙二胺、二曱基曱醯胺、三乙醇胺或二乙醇胺,。然而，溶劑之選 擇並不限於上述提及之醇類、醚類或酮類溶劑，只要是能將上述 〇 化合物溶解之单一或混合溶劑皆可。 於一實施例中，混合氯化銅（011(::12)與氯化銦（Incl3)於水溶液 中，即可製得步驟（a)之溶液。 此外，步驟（a)之溶液尚可添加其它離子，以改善太陽電池之 特性。例如，可添加IA族化合物提高電池之光電轉化效率，其 中I A族包括鐵）’麵（Na)、鉀（κ)或上述之組合，而I a族之化 合物包括I A族之ii化物、硝酸物、醋酸物、硫酸物、碳酸物或 氯酸物，例如氯化鋰(LlCl)、氯化鈉（NaCl)、氯化鉀（KC1)、硝酸鋰 Q (LiN〇3)、硝酸鈉(NaN03)、硝酸鉀（kn〇3)、醋酸鋰（CH3c〇〇Li)、 醋酸鈉（CH3COONa)、醋酸鉀（CH3C〇〇K)、硫酸鐘（Li2S〇4)、硫酸 納（NaAO4)、硫酸鉀dSO4)、碳酸鋰(Li2c〇3)、碳酸鈉（Na2C〇3)、 碳酸鉀（KsCO3)、氯酸鋰（LiCl〇3)、氯酸鈉（NaC103)或氯酸鉀 (KCIO3)。而前驅物與IA族之莫耳數比為約（1〇〜2〇〇〇) : 1。 再者’步驟⑷之洛液尚可添加聚合劑（p〇lymerizati〇n agent) 於溶劑中，聚合劑之作用在於維持溶液中陽離子之分散均勻性， 而聚合劑之種類包括乙二胺四乙酸（ethylenediaminetetraacetic acid，EDTA)、乙二醇（ethylene giyC〇i)、聚乙二醇（polyethylene 6 201100330 glycol)、聚乙烯醇(polyvinyl alcohol)、檸1樣酸（citric acid)、草酸 (oxalic acid)、丙酸(propionic acid)、酒石酸（tartaric acid)、順丁烯 二酸(maleic acid)或上述之組合。 接著，進行步驟(b)，將步驟（a)之混合物進行乾燥或沉澱步驟 以獲得含有I B族、Π A族之前驅物（precursor)，其中乾燥步驟包 括低溫乾燥、紅外線加熱、微波加熱法或冷凉乾燥法。於一實施 例中，沉殿步驟係指加入驗性溶液（例如氫氧化納）於上述溶液中， 使I B族、Μ A族離子沉澱，而得到含有I B族、]Π A族之前驅物， 其中驗性溶液之pH値大於約8，較佳大於約10。 Ο 此處需注意的是，本發明先將IB族、HA族化合物溶解之 後再乾燥，相較於習知技術（製備I B族、ΠΑ族之合金），能得到 顆粒小且均勻之前驅物。 之後5進行步驟（c)之前，亦即步驟（b)之後尚包括過濾並乾燥 前驅物。過濾時可使芾去離子水重複清洗，以得到較純之固體。 乾燥方法例如低溫乾燥、紅外線加熱、微波加熱法或冷凍乾燥法。 然而，並不限於上述提及之方法，只要能將溶劑完全去除即可。 此外，亦可不進行此過濾、乾燥步驟，直接進行步驟（c)。再者，由 Q 於反應的過程中可能產生許多有機物，為了避免有機物的干擾， 除上述過濾乾燥前驅物之外，也可單純利用加熱法排除前驅物中 的有機物。 接著，進行步驟（c)，將含有VIA族化合物之溶液或粉末與前 驅物混合，其中VIA族包括硫（S)、硒（Se)、銻（Te)或上述之組合， 而VIA族化合物包括含有VIA族之氧化物、鹵化物、鹵氧化物、 硫化物、砸化物、胺化物、脲化物、砸酸物、硫酸物或蹄酸物， 例如氧化站（Se〇2)、氧化碲（Te〇2)、硫酸(H2S〇4)、砸酸(H2Se〇4)、 碲酸(H2Te04)、亞硫酸(H2S03)、亞硒酸(H2Se03)、亞碲酸(H2Te03)、 7 201100330 硫腺（thiourea, CS(NH2)2)、石西脲（selenourea, CSe(NH2)2)、二氯化石西 (SeCl2)、四氯化硒（SeCl4)、二氯化碲（TeCl2)、四氯化碲（TeCl4)、 二漠化砸（SeBr2)、四漠化砸（SeBr4)、二溴化碲（TeBrd、四漠化碲 (TeBr4)、氯氧化硒（SeOCl2)或硫化硒（SeS2)。上述含有VIA族化合 物之溶液或固體與前驅物之莫耳數比為約（〇· 1〜20) : 1，較佳為 (0.1 〜15) : 1，更佳為（0.1 〜10) : 1。 於一實施例中，VIA族化合物與前驅物莫耳數比為10 : 1， 利甩球磨的方式，均勻的混合兩者。 此處應注意的是，由於習知技術中大多利用真空製程（亦即通 〇 入含有VIA族氣體）進行熱處理，然而，通入氣體時，反應僅會發 生於前驅物的表面，使得前驅物之底層無法與VIA族氣體接觸· 因而無法得到均勻的黃銅礦化合物，因此，本發明利用含有VIA 族之溶液或粉末進行反應，可使\ΊΑ族化合物與前驅物均勻的混 合，使反應更加完全。 上述步驟（a)〜步驟（c)之製備過程，可於一般室溫與大氣環境 下進行，不需額外控制製程之氣氛、溫度、濕度與壓力。 接著進行步驟（d)，將步驟（c)之混合物進行熱處理，其中熱處 Q 理係於含有下列氣體的氣氛下進行：氮氣（N2)、氫氣（H2)、氬氣 (Ar)、一氧化碳(CO)、二氧化碳（C02)、氨氣(NH3)、一氧化氮(NO) 或上述之組合。 上述熱處理之溫度為約300°C〜700°C，較佳為約400°C〜600 °C，而熱處理之時間為約0.1小時〜48小時，較佳為約0.3小時 〜24小時，最佳為0.5小時〜18小時。然而，上述溫度可設計成溫 度梯度（temperature gradient)，可依據欲得到之黃銅礦粉末顆粒大 小對溫度作適當的調控。熱處理中控制升溫、降溫速度可得更佳 品質之粉末，升溫及降溫之速度為約0.3〜100 (°C/分鐘），較佳為 8 201100330 〇·5〜5〇(°C/分鐘）’更佳為1〜30fC/分鐘）。 此外’為使VIA族化合物之提供更完全，除上述氣體外，尚 可另卜提i、D有VIA族之氣體，例如硒化氫(Hje)、硫化氫田j)、 砸（Se)蒸氣、硫⑻蒸氣、蹄(Te)蒸氣或上述之組合。 卜本卷明另外提供黄銅礦（chalcopyrite)粉末製法之第二 實施例’其包括以下步驟：⑷混合含有IB族、A族與似： 之,合物於-溶劑中，其中m族、族與似族之莫耳數比為 (0./ 1. .) ’（0.7〜1.4) : (〇1〜2〇)，較佳為（〇 8〜13) : m) ❹ (0.1〜15) ’最佳為㈣〜1‘2):叫1_2) : (0.1,。上述ίΒ族化合 矢化s物族化合物與溶劑之種類皆與第一實施例 相同，在此不再贅述。 、 〜 '妾_5、厅^ ’驟⑼’將女驟⑷之溶液進行乾燥或沉题步驟以獲 仵“ IB知、族與VIA族之前黑物(precurs〇r)，里中 與過濾之方法同於第—實施例。 ，’、〜小 之後，進行步驟⑷，將步驟⑼之前驅物進行熱處理以得列兮 處理之方法、時間與溫度皆可與第-細 π目同，在此个再資逑。 第二實施例與第-實施例之主要差別在於，於步驟⑷中，先 將^族之化合物與ΙΒ族、ΗΑ族一起混合，因此，第 之優點在於可以能更節省製作纟车 、q 太⑽心廿㈣，且同樣可獲得均勻粉體。201100330 VI. Description of the Invention: [Technical Field of the Invention] The present invention relates to a method of fabricating a semiconductor material, and more particularly to a method for producing a chalcopyrite powder. • [Prior Art] Semiconductor materials have a unique band gap that can change the energy gap of a semiconductor by regulating the composition of the material, so it can be applied as a light absorbing layer of a photoelectronic device. . Among the various semiconductor materials, among them, the I Β-ΠΑ-VIA compound having a chalcopyrite structure is particularly valued, and it can be used as a film for a copper indium gallium selenide battery (Cu(In, Ga). Se2, CIGS), and has a good photoelectric conversion efficiency. At present, the method for producing a film of a c. halcopyrite compound can be divided into a vacuum and a non-vacuum process, and the vacuum process includes a co-evaporation, a sputtering process, and the like, and the vacuum process includes electricity. Electrodeposition, electrodeless electroless (electroless), coating process or chemical spray p3 (rolysis), because the cost of the vacuum process is expensive with the equipment, and it is only It can be applied to small-scale photovoltaic elements and cannot be applied to large-sized components. Therefore, development of non-vacuum technology has begun. The preparation method of the early non-vacuum process is to deposit metal ions of group IB and lan on the substrate respectively, and after reduction to metal, and then subjected to selenization heat treatment to obtain chalcopyrite compound, however, the melting point of the 1 lan metal is lower. During the heat treatment process, it will aggregate due to melting, and thus a non-uniform film will be obtained. In order to obtain a more uniform film, development of various chalcopyrite compounds has begun. US Pat. No. 5,445,847 discloses a method for preparing a chalcopyrite compound 201100330. First, the IB powder and the HA powder are mixed, followed by ball milling and mixing, and then sent to a high temperature sintering to obtain an I Β-ΠΙ Α oxide, and finally A chalcopyrite compound can be obtained by heat treatment in a gas containing Group VIA. US 6,268,014 discloses a method for preparing a chalcopyrite compound by first preparing IB-bismuth oxide particles, which are then deposited on a substrate by spraying, and then subjected to heat treatment in a gas containing Group VIA to obtain yellow. Copper ore compound. In summary, if a powder of a small and uniform chalcopyrite compound can be produced, the powder is slurried and a uniform film can be produced by the coating process. SUMMARY OF THE INVENTION The present invention provides a method for preparing a chalcopyrite powder, comprising the steps of: (a) mixing a compound containing a group IB and a steroid in a solvent; (b) preparing the solution of the step (a) Performing a drying or sinking step to obtain a precursor containing Group IB, Group IE A; (c) mixing a solution or powder containing a Group VIA compound with the precursor; and (d) taking the step ( The mixture of c) is subjected to heat treatment to obtain the chalcopyrite powder. The invention further provides a method for preparing a chalcopyrite powder, comprising: ◎ the following steps: (a) mixing a compound containing a group IB, a steroid and a group VIA in a solvent; (b) a solution of the step (a) A drying or precipitation step is performed to obtain a precursor containing Group IB, Group IIA and Group VIA; and (c) heat treatment is performed on the precursor of step (b) to obtain the chalcopyrite powder. The above and other objects, features and advantages of the present invention will become more <RTIgt; A method for preparing a chalcopyrite powder, comprising the steps of: first performing step (a) 'mixing a compound containing a group IB and a lanthanide A ion into a granule", wherein IB comprises copper (Cu), silver (Ag) ), gold (Au) or a combination thereof, and the compound of Group IB includes an oxide, a nitride, a cerium oxide, a halide, a nitrate, an acetic acid, a sulfate, a carbonate, a gas acid, Filling acid, citrate, oxalic acid, fillers such as copper oxide (CuO), copper nitride (Cu(N3)2), copper hydroxide (Cu(OH)2), copper chloride (CuCl2), Silver nitrate (AgN03), copper nitrate (Cu(N03)2), copper sulfate (CuS〇4), copper acetate (Cu(CH3COO)2), silver acetate (CH3COOAg), copper carbonate (Cu2C03), copper oxalate (CuC204) Copper chlorate O (Cu(C104)2), copper phosphate (Cu3(P04)2), copper selenate (CuSe04) or copper phosphide (Cu3P). ΠΙ Group A includes Ming (A1), Indium (In), Gallium (Ga) or a combination of the above, and Group A compounds include oxides, nitrides, hydroxides, compounds, nitrates, acetates containing HA groups. , sulphate, carbonate, chlorate, phosphate, selenate 'oxalate or phosphide, such as indium oxide (In2〇3), gallium oxide (Gar〇3), indium nitride (InN), nitriding Gallium (GaN), indium hydroxide (ln(〇H)3), barium hydroxide (Ga(〇H)3), aluminum chloride (A1C13), indium chloride (InCl3), gallium chloride (GaCl3), Aluminum nitrate (A1(N03)3), succinium indium (In(N〇3)3), sulphate (Ga(N〇3)3), indium acetate (ln(CH3COO)3), cool Q acid (A1(CH3C00)3), aluminum carbonate (Al2(C〇3)3), aluminum oxalate (Al2(C2〇4)3), gallium acetate (Ga(CH3COO)3), indium sulfate (ln2(s〇4) 3), aluminum sulfate (Al2(s〇4)3), gallium sulfate (GaKSOO3), indium chlorate (In(C104)3), gallium chlorate (Ga(ci〇4)3), indium phosphate (ΙηΡ04) ), gallium phosphate (GaP04), indium selenate (In2 (Se〇4) 3), gallium selenate (Ga 2 (Se04) 3), phosphating! (InP) or gallium arsenide (GaP). The molar ratio of the Group IB and the Group HIA compound of the step (a) is about (〇7 to 14): (0.7 to 1.4)' is preferably about (0.8 to 1.3): (0.8 to 1.3), preferably About (〇.8~1.2): (0'8~1.2). The selection of the I B group and the steroid compound is not limited to the above-mentioned compound 5 201100330, as long as the compound containing the ib group and the Ha group element is acceptable. The solvent includes water, an acid, a base, an alcohol, a ketone, an ether, an amine or other organic solvent, and the solvent is a non-toxic general solvent, wherein the acid includes nitric acid, hydrochloric acid, sulfuric acid, acetic acid or pyruvic acid; The class includes sodium hydroxide solution or citric acid solution, ammonia water; alcohols include decyl alcohol, ethanol, propanol, isopropanol, n-butanol, isoamyl alcohol or ethylene glycol; ketones include acetone, methyl ethyl ketone, methyl Isobutyl ketone; ethers include oxime ether, diethyl ether, methyl ethyl ether, monophenyl ether, ethylene glycol oxime ether butanol or ethylene glycol acetic acid; amines including ethylene diamine, dimethyl decylamine, triethanolamine Or diethanolamine,. However, the solvent is not limited to the above-mentioned alcohol, ether or ketone solvent as long as it is a single or mixed solvent capable of dissolving the above hydrazine compound. In one embodiment, the solution of the step (a) can be prepared by mixing copper chloride (011 (:: 12) and indium chloride (Incl3) in an aqueous solution. Further, the solution of the step (a) can be added. Other ions to improve the characteristics of the solar cell. For example, a group IA compound may be added to improve the photoelectric conversion efficiency of the battery, wherein the group IA includes iron) 'face (Na), potassium (κ) or a combination thereof, and the group I a The compound includes a Group IA compound, a nitrate, an acetate, a sulfate, a carbonate or a chloric acid, such as lithium chloride (LlCl), sodium chloride (NaCl), potassium chloride (KC1), lithium nitrate Q ( LiN〇3), sodium nitrate (NaN03), potassium nitrate (kn〇3), lithium acetate (CH3c〇〇Li), sodium acetate (CH3COONa), potassium acetate (CH3C〇〇K), sulfuric acid clock (Li2S〇4) , sodium sulphate (NaAO4), potassium sulfate dSO4), lithium carbonate (Li2c〇3), sodium carbonate (Na2C〇3), potassium carbonate (KsCO3), lithium chlorate (LiCl〇3), sodium chlorate (NaC103) or Potassium chlorate (KCIO3). The molar ratio of the precursor to the IA group is about (1〇~2〇〇〇): 1. Further, the step (4) can also add a polymerization agent (p〇lymerizati〇n agent) in a solvent, and the polymerization agent functions to maintain the uniformity of dispersion of the cation in the solution, and the type of the polymerization agent includes ethylenediaminetetraacetic acid. (ethylenediaminetetraacetic acid, EDTA), ethylene glycol (ethylene giyC〇i), polyethylene glycol (polyethylene 6 201100330 glycol), polyvinyl alcohol (polyvinyl alcohol), citric acid, oxalic acid , propionic acid, tartaric acid, maleic acid or a combination thereof. Next, step (b) is carried out, and the mixture of step (a) is subjected to a drying or precipitation step to obtain a precursor containing Group IB, Group A, wherein the drying step comprises low temperature drying, infrared heating, microwave heating or Cool and dry method. In one embodiment, the sinking step refers to adding an inert solution (for example, sodium hydroxide) to the above solution to precipitate IB group and ΜA group ions, thereby obtaining a precursor containing IB group, ΠA group, Wherein the pH of the test solution is greater than about 8, preferably greater than about 10.此处 It should be noted here that the present invention first dissolves the Group IB and the HA compound and then dries it. Compared with the conventional technique (preparation of the Group I B, the alloy of the lanthanum), a small and uniform precursor can be obtained. Subsequent to step 5 (c), step (b) is followed by filtration and drying of the precursor. The deionized water can be repeatedly washed during filtration to obtain a relatively pure solid. Drying methods such as low temperature drying, infrared heating, microwave heating or freeze drying. However, it is not limited to the above-mentioned method as long as the solvent can be completely removed. Further, the step (c) may be directly carried out without performing the filtration and drying steps. Further, a large amount of organic matter may be generated during the reaction of Q, and in order to avoid interference of organic substances, in addition to the above-mentioned filter drying precursor, the organic matter in the precursor may be removed by heating alone. Next, step (c) is carried out to mix a solution or powder containing a compound of the VIA group with a precursor, wherein the group VIA comprises sulfur (S), selenium (Se), tellurium (Te) or a combination thereof, and the group VIA compound includes Containing oxides, halides, oxyhalides, sulfides, tellurides, aminides, ureas, citrates, sulfates or humic acids of Group VIA, such as oxidation stations (Se〇2), cerium oxide (Te) 〇2), sulfuric acid (H2S〇4), citric acid (H2Se〇4), citric acid (H2Te04), sulfite (H2S03), selenite (H2Se03), phthalic acid (H2Te03), 7 201100330 sulphur gland ( Thiourea, CS(NH2)2), selenourea, CSe(NH2)2, SeCl2, SeCl4, TeCl2, Tetrachloride (TeCl4), Se2 (SeBr2), SeBr4, SeB4, TeBrd, TeBr4, SeOCl2 or SeS2. The ratio of the molar ratio of the solution or solid of the VIA group compound to the precursor is about (〇·1 to 20): 1, preferably (0.1 to 15): 1, more preferably (0.1 to 10): 1. In one embodiment, the VIA family The molar ratio of the compound to the precursor is 10:1, the method of the ball milling, the uniform mixing of the two. It should be noted here that most of the prior art utilizes a vacuum process (ie, through the VIA) The gas is heat-treated. However, when the gas is introduced, the reaction only occurs on the surface of the precursor, so that the underlayer of the precursor cannot be in contact with the Group VIA gas, and thus a uniform chalcopyrite compound cannot be obtained. Therefore, the present invention utilizes The reaction of the solution or powder containing the VIA group can uniformly mix the steroid and the precursor to make the reaction more complete. The preparation process of the above steps (a) to (c) can be carried out at room temperature and atmospheric environment. The process is carried out without additional control of the atmosphere, temperature, humidity and pressure of the process. Next, step (d) is carried out, and the mixture of the step (c) is subjected to heat treatment, wherein the heat is carried out in an atmosphere containing the following gas: nitrogen (N2), hydrogen (H2), argon (Ar), carbon monoxide (CO), carbon dioxide (C02), ammonia (NH3), nitrogen monoxide (NO) or a combination thereof. The temperature of the above heat treatment is It is about 300 ° C to 700 ° C, preferably about 400 ° C to 600 ° C, and the heat treatment time is about 0.1 hour to 48 hours, preferably about 0.3 hour to 24 hours, preferably 0.5 hour to 18 hours. However, the above temperature can be designed as a temperature gradient, and the temperature can be appropriately adjusted depending on the size of the chalcopyrite powder to be obtained. In the heat treatment, the temperature of the heating and the cooling rate can be controlled to obtain a better quality powder, and the heating and cooling speed is about 0.3 to 100 (° C./min), preferably 8 201100330 〇·5 to 5 〇 (° C/min). More preferably 1 to 30 fC / min). In addition, in order to make the supply of the VIA compound more complete, in addition to the above gases, it is possible to add a gas of Group VIA, such as hydrogen selenide (Hje), hydrogen sulfide field j, and cesium (Se) vapor. Sulfur (8) vapor, hoof (Te) vapor or a combination thereof. A second embodiment of a chalcopyrite powder process is additionally provided, which comprises the following steps: (4) mixing contains a group IB, a group B, and a compound in a solvent, wherein the group m, the group The ratio of the molar ratio to the like family is (0./ 1. .) '(0.7~1.4) : (〇1~2〇), preferably (〇8~13) : m) ❹ (0.1~15) 'Best is (4) ~ 1'2): is called 1_2): (0.1, The above-mentioned Β 化 矢 s s s s s s s s s s s s s s s s s s s s s s s s s s s s s s s s s s s s s妾_5, 厅^ 'Sudden (9)' Dry or the solution of the solution of the female (4) to obtain the "precurs〇r" of the IB, family and VIA, the same as the filtration method First-example. After ',~ is small, step (4) is carried out, and the method of heat treatment of the precursor before step (9) is carried out to obtain the method of treatment, and the time and temperature can be the same as the first-thin π. The main difference between the second embodiment and the first embodiment is that in the step (4), the compound of the group is first mixed with the steroid and the steroid, and therefore, the first advantage is that More savings in the production of brakes, q too (10) heart (4), and also get a uniform powder.
Ω1 恤)粉末，其顆粒大小W 且由掃描式電子顯微鏡(= 2=二=黃銅礦粉末顆粒均勻。另外，由X光繞射圖譜 二二 Γ之1 B-mA-VIA族化合物，證實產物為黃銅鑛 (chalcopyrite)之晶體結構。 、广' 綜上所述，本發明製備黄銅確咖叫她)粉末之方法具有 201100330 下述優點： (1) 相較於習知之合金製程，可得到顆粒小且均勻之I B-IHA 月|J驅物， (2) 相較於習知之氣體硒化步驟，本發明利用溶液或粉末的 VIA族化合物，可使VIA族化合物與前驅物之反應更完全； (3) 製備方式簡單且便宜，且黃銅礦粉末顆粒小且均勻，未 來具有量產潛力。 由上述製法製得之黄銅礦粉末，其顆粒小且均勻，可作為真 空製程之乾材（target)，其中真空製程包括蒸鐘或漉鐘。 〇 此外，上述黃銅礦粉末製成漿料（Slurry)後，可作為塗佈製程 之原料，其中塗佈製程包括旋轉塗佈（spin coating)、棒狀塗佈（bar coating)、浸潰塗佈（dip coating)、滾筒塗佈（roll coating)、喷霧塗 佈（spray coating)、凹版式塗佈（gravure coating)、喷墨印刷（ink: jet printing)、狭缝塗佈（slot coating)或刮刀塗佈（Made coating)。再者； 黄銅礦粉末亦可作為太陽能電池（Solar Cell)之吸光材料。 【實施例】 0 實施例1 依CuInSe2化學成分比例，配出CuCl2和InCb混合之水溶液， 並將此水溶液缓慢滴入pH=9之NaOH水溶液當中，過濾出沉殿物 後並乾燥，將乾燥後的沉殿物和過量的砸粉進行球磨混合，使Se 與（Cu2++In3+)之莫耳數比為10: 1，然後在氮氫混合的氣氛下500°C 加熱一小時，即可獲得所需的CuInSe2粉體。 此粉體經X-ray繞射圖譜分析後可發現有（112)、（204)/(220)、 與（312)/(116)三支主要繞射峰，其中（204)與（220)為同位置之繞射 鋒，（312)與（116)亦為同位置之繞射鋒，符合ICDD卡編號89-5649 10 201100330 圖譜，此粉體為黃銅礦結構。經SEM分析，得知粉體大小為約0.5 μΐΉ，且粉體型態均一。 實施例2 依 CuIn0.3Ga0.7Se2 化學成分比例，配出 CuCl2、I11CI3、Ga(N03) 3與Se〇2混合之水溶液，並加入5莫耳％的NaCl水溶液，加熱乾 燥後，將乾燥的沉澱物磨粉，然後在含涵氣的氫氧氣氛下550°C 加熱三十分鐘，即可獲得所需的CuInQ.3GG.7Se2粉體。 此粉體經；X-ray繞射圖譜分析後可發現有（112)、（204)/(220)、 〇 與（312)/(116)三支主要繞射峰，其中（204)與（220)為同位置之繞射 鋒，（3 12)與（116)亦為同位置之繞射鋒，證實此粉體為黃銅礦結構。 實施例3 依 CuIn0.7Ga0.3Se.2 化學成分比例；配出 CuC12、InCh 與 Ga(N〇3)3 混合之乙醇溶液，加熱乾燥後，將乾燥後的沉殿物和過量的砸粉 進行球磨混合，使Se與（Cinln。’+Ga'i)之莫耳數比為0.2 : 1 ’然 後在含硒氣的氮氫氣氛下550°C加熱30分鐘，即可獲得所需的 ❾ CuInG.7Gao.3Se2 粉體。 此粉體經X-ray繞射圖譜分析後可發現有（112)、（204)/(220)、 與（312)/(116)三支主要繞射峰，其中（204)與（220)為同位置之繞射 鋒，（3 12)與（116)亦為同位置之繞射鋒，符合ICDD卡編號35-1102 圖譜，證實此粉體為黃銅礦結構。 實施例4 依CiiuAlSes化學成分比例，配出CuCl2和A1(N03)3混合之乙 二醇單曱醚（ethyleneglycol monomethyl ether)溶液，.並加入 10 11 201100330 mole%的NaCl和過量的石西酸，使Se离隹子與（Cu2++A13 )之莫耳數比 為10 : 1，將此溶液乾燥，乾燥後之乾燥物，在氮氣氣氛下450°C 加熱一小時，即可獲得所需的Cuh2AlSe2粉體。 此粉體經X-ray繞射圖譜分析後可發現有（112)、（204)/(220)、 與（312)/(116)三支主要繞射峰，其中（204)與（220)為同位置之繞射 鋒，（312)與（116)亦為同位置之繞射鋒，符合ICDD卡編號75-0101 圖譜’證貫此粉體為黃銅礦結構。 實施例5 ❹ 依Cu〇.8GaSeS化學成分比例，配出CuCh和Ga(N03)3混合之 硝酸水溶液，並加入10莫耳％的KC1後將此溶液乾燥，將乾燥後 的乾燥物和過量的砸粉與硫粉進行球磨混合，使（Se+S)與 (Cu2++In3]之莫耳數比為5 : 1，然後在氮氫氣氛下450°C加熱一 小時，即可獲得所需的Cu〇GaSeS粉體。 此粉體經X-ray繞射圖譜分析後可發現有（112)、（204)、與（3 12) 三支主要繞射峰，符合ICDD卡編號36-1312圖譜，證實此粉體為 黃銅礦結構。 實施例6 依Agings]化學成分比例，配出AgN03和In(N〇3)3之混合水 溶液，並將此水溶液缓慢滴入K0H水溶液當中，過濾出沉殿物後 並乾燥，將乾燥後的沉殿物和過量的石西粉進行球磨混合，使S與 (Ag++In3+)之莫耳數比為3 : 1，然後在真空氣氛下500°C加熱三十 六小時，即可獲得所需的Agln^S〗粉體。 此粉體經X-ray繞射圖譜分析後可發現有（110)、（121)兩支主要 繞射峰，符合ICDD卡編號75-2379圖譜，證實此粉體為黃銅礦結 12 201100330 構0 實施例7 依CuInSk化學成分比例，配出CuCh和Inch之混合水溶液， 再加入；1=争核酸（citric acid)及乙二醇（ethylene glycol)當作今人列 (polymerization agent)。 〇 將此水溶液攪拌均勻後進行乾燥，乾燥後於5〇〇。€加熱—小時 排除有機物以獲得前驅物，將前驅物與過量的硒粉進行球磨混 與(Cu、3’之莫耳數比為10:1，然後在氮氫混：: …—小k 即可獲得所需的CuInSe2粉體。 ⑶:===分:Γ 發現有(112)、(2。4)_ 峰仰卿物 圖譜，此粉體為黃鋼礦結構。 一 ^編遽㈣4d 定本個f佳實施例揭露如上’然其並非用以限 明之精神和範_領射具有料知識者，在不脫離本發 護範圍當視後附田可作任意之更動與潤飾，因此本發明之保 申請專利範圍所界定者為準。 33 201100330 【圖式簡單說明】 第1圖為一 X-ray繞射圖，用以說明本發明之黃銅礦粉末之 結構。 【主要元件符號說明】 •fe 〇 /Ω1 shirt) powder, its particle size W and by scanning electron microscopy (= 2 = two = chalcopyrite powder particles uniform. In addition, by the X-ray diffraction pattern of bismuth 1 B-mA-VIA compound, confirmed The product is the crystal structure of chalcopyrite. In the above, the method for preparing the powder of the present invention has the following advantages: (1) Compared with the conventional alloy process, A small and uniform particle of I B-IHA is obtained, and (2) the present invention utilizes a solution or powder of a Group VIA compound to react a VIA compound with a precursor compared to a conventional gas selenization step. More complete; (3) The preparation method is simple and cheap, and the chalcopyrite powder particles are small and uniform, and have potential for mass production in the future. The chalcopyrite powder obtained by the above method has small and uniform particles and can be used as a dry target of a vacuum process, wherein the vacuum process includes a steam clock or a cuckoo clock. Further, after the above-mentioned chalcopyrite powder is made into a slurry, it can be used as a raw material for a coating process, wherein the coating process includes spin coating, bar coating, and dip coating. Dip coating, roll coating, spray coating, gravure coating, ink: jet printing, slot coating Or Made coating. Furthermore, chalcopyrite powder can also be used as a light absorbing material for solar cells. EXAMPLES Example 1 According to the chemical composition ratio of CuInSe2, an aqueous solution of CuCl2 and InCb was mixed, and the aqueous solution was slowly dropped into a NaOH aqueous solution of pH=9, and the precipitate was filtered and dried, and dried. The sediment and the excess tantalum powder are ball-milled and mixed so that the molar ratio of Se to (Cu2++In3+) is 10:1, and then heated at 500 ° C for one hour in a nitrogen-hydrogen mixed atmosphere. The required CuInSe2 powder. The powder was analyzed by X-ray diffraction and found to have three main diffraction peaks (112), (204)/(220), and (312)/(116), of which (204) and (220) For the diffraction position of the same position, (312) and (116) are also the diffraction fronts of the same position, which conforms to the ICDD card number 89-5649 10 201100330 map, and the powder is a chalcopyrite structure. After SEM analysis, it was found that the powder size was about 0.5 μΐΉ, and the powder type was uniform. Example 2 According to the chemical composition ratio of CuIn0.3Ga0.7Se2, an aqueous solution of CuCl2, I11CI3, Ga(N03) 3 and Se〇2 was prepared, and a 5 mol% NaCl aqueous solution was added thereto, and after heating and drying, the dried precipitate was dried. The powder was ground and then heated at 550 ° C for 30 minutes in a hydrogen-containing atmosphere containing a gas to obtain the desired CuInQ.3GG.7Se2 powder. After the X-ray diffraction pattern analysis, there are three main diffraction peaks (112), (204)/(220), 〇 and (312)/(116), of which (204) and 220) is the diffraction front of the same position, and (3 12) and (116) are also the diffraction fronts of the same position, confirming that the powder is a chalcopyrite structure. Example 3 According to the chemical composition ratio of CuIn0.7Ga0.3Se.2; the ethanol solution mixed with CuC12, InCh and Ga(N〇3)3 was prepared, and after heating and drying, the dried sediment and excess strontium powder were subjected to drying. The ball mill is mixed so that the molar ratio of Se to (Cinln.'Ga'i) is 0.2:1 ' and then heated at 550 ° C for 30 minutes under a nitrogen-hydrogen atmosphere containing selenium gas to obtain the desired ❾ CuInG .7Gao.3Se2 powder. The powder was analyzed by X-ray diffraction and found to have three main diffraction peaks (112), (204)/(220), and (312)/(116), of which (204) and (220) For the diffraction position of the same position, (3 12) and (116) are also the diffraction fronts of the same position, which conforms to the ICDD card number 35-1102 map, confirming that the powder is a chalcopyrite structure. Example 4 According to the ratio of CiiuAlSes chemical composition, a solution of ethyleneglycol monomethyl ether mixed with CuCl2 and A1(N03)3 was added, and 10 11 201100330 mole% NaCl and excess amount of stacinic acid were added. The molar ratio of Se to (Cu2++A13) is 10:1, the solution is dried, and the dried product is dried, and heated at 450 ° C for one hour in a nitrogen atmosphere to obtain the desired Cuh2AlSe2 powder. The powder was analyzed by X-ray diffraction and found to have three main diffraction peaks (112), (204)/(220), and (312)/(116), of which (204) and (220) For the same position of the diffraction front, (312) and (116) are also the same position of the diffraction front, in line with ICDD card number 75-0101 map 'certified that this powder is a chalcopyrite structure. Example 5 配 According to the chemical composition ratio of Cu〇.8GaSeS, an aqueous solution of nitric acid mixed with CuCh and Ga(N03)3 was added, and after adding 10 mol% of KC1, the solution was dried, and the dried product and excess were dried. The ball powder is mixed with the sulfur powder by ball milling, so that the molar ratio of (Se+S) to (Cu2++In3) is 5:1, and then heated at 450 ° C for one hour in a nitrogen-hydrogen atmosphere to obtain the desired Cu〇GaSeS powder. This powder can be found by X-ray diffraction pattern, and there are three main diffraction peaks (112), (204), and (3 12), which conform to the ICDD card number 36-1312 map. It was confirmed that the powder was a chalcopyrite structure. Example 6 According to the chemical composition ratio of Agings, a mixed aqueous solution of AgN03 and In(N〇3)3 was prepared, and the aqueous solution was slowly dropped into an aqueous solution of K0H, and filtered. After the temple is dry and dry, the dried Shen Temple and the excess Shixi powder are ball milled, so that the molar ratio of S to (Ag++In3+) is 3:1, then 500 °C in a vacuum atmosphere. After heating for 36 hours, the desired Agln^S powder can be obtained. After the X-ray diffraction pattern analysis, the powder can be found to have two main (110) and (121) The diffraction peak conforms to the ICDD card number 75-2379 map, confirming that the powder is a chalcopyrite junction 12 201100330. Structure 0 Example 7 According to the chemical composition ratio of CuInSk, a mixed aqueous solution of CuCh and Inch is added, and then added; Citric acid and ethylene glycol are used as the polymerization agent. 〇 The aqueous solution is stirred uniformly, dried, and dried at 5 〇〇. Heating-hours to remove organic matter to obtain precursors The precursor is mixed with an excess amount of selenium powder by ball milling (the molar ratio of Cu to 3' is 10:1, and then the desired CuInSe2 powder can be obtained by mixing nitrogen and hydrogen: : ... - small k. (3) :===分:Γ Found (112), (2. 4) _ Feng Yangqing map, this powder is a yellow steel structure. A ^ braided (four) 4d fixed this example of a good example of the above It is not intended to limit the spirit and scope of the _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ [Simple diagram of the figure] Figure 1 is an X-ray diffraction pattern for Chalcopyrite structure bright powder of the present invention. The main element symbol square DESCRIPTION • fe /
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| TW098121317A TW201100330A (en) | 2009-06-24 | 2009-06-24 | Fabrication method for chalcopyrite powder |
| US12/813,403 US8057781B2 (en) | 2009-06-24 | 2010-06-10 | Fabrication method for chalcopyrite powder |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI469918B (en) * | 2011-01-13 | 2015-01-21 | Method for making a chalcopyrite-type compound | |
| CN112047309A (en) * | 2020-08-21 | 2020-12-08 | 广东先导稀贵金属材料有限公司 | A kind of production method of selenium disulfide powder |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US8501524B2 (en) * | 2010-02-26 | 2013-08-06 | Electronics And Telecommunications Research Institute | Method of manufacturing thin-film light-absorbing layer, and method of manufacturing thin-film solar cell using the same |
| WO2013033729A1 (en) * | 2011-09-02 | 2013-03-07 | Alliance For Sustainable Energy, Llc | Electrodepostion of gallium for photovoltaics |
| US9573809B2 (en) * | 2012-03-30 | 2017-02-21 | Micron Technology, Inc. | Method of forming a metal chalcogenide material and methods of forming memory cells including same |
| US8231848B1 (en) * | 2012-04-10 | 2012-07-31 | Sun Harmonics Ltd | One-pot synthesis of chalcopyrite-based semi-conductor nanoparticles |
| US20140256082A1 (en) * | 2013-03-07 | 2014-09-11 | Jehad A. Abushama | Method and apparatus for the formation of copper-indiumgallium selenide thin films using three dimensional selective rf and microwave rapid thermal processing |
| CN109817734A (en) * | 2018-12-26 | 2019-05-28 | 北京铂阳顶荣光伏科技有限公司 | A kind of preparation method of copper-indium-galliun-selenium film solar cell absorbed layer |
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| EP0574716B1 (en) * | 1992-05-19 | 1996-08-21 | Matsushita Electric Industrial Co., Ltd. | Method for preparing chalcopyrite-type compound |
| US6268014B1 (en) * | 1997-10-02 | 2001-07-31 | Chris Eberspacher | Method for forming solar cell materials from particulars |
| TWI421214B (en) * | 2008-12-03 | 2014-01-01 | Ind Tech Res Inst | IBIIIAVIA family amorphous phase compound and method for producing IBIIIAVIA family amorphous phase precursor applied to thin film solar cell |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| TWI469918B (en) * | 2011-01-13 | 2015-01-21 | Method for making a chalcopyrite-type compound | |
| CN112047309A (en) * | 2020-08-21 | 2020-12-08 | 广东先导稀贵金属材料有限公司 | A kind of production method of selenium disulfide powder |
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| US8057781B2 (en) | 2011-11-15 |
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